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On the appearance of nitrite anion in [PdX(OAc)L2] and [Pd(X)(C∧N)L] syntheses (X = OAc or NO2): Photocrystallographic identification of metastable Pd(η1-ONO)(C∧N)PPh3


Reference:

Bajwa, S. E., Storr, T. E., Hatcher, L. E., Williams, T. J., Baumann, C. G., Whitwood, A. C., Allan, D. R., Teat, S. J., Raithby, P. R. and Fairlamb, I. J. S., 2012. On the appearance of nitrite anion in [PdX(OAc)L2] and [Pd(X)(C∧N)L] syntheses (X = OAc or NO2): Photocrystallographic identification of metastable Pd(η1-ONO)(C∧N)PPh3. Chemical Science, 3 (5), pp. 1656-1661.

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    Official URL:

    http://dx.doi.org/10.1039/c2sc01050j

    Abstract

    Pd 3(OAc) 5NO 2, an impurity in "Pd(OAc) 2" {formally Pd 3(OAc) 6}, emerges as a serious issue in the synthesis of pure Pd II complexes derived from Pd(OAc) 2, for example in our C-H activation precatalyst, Pd(OAc) 2(pip) 2 (pip = piperidine). A previous proposal that nitrite anion can be formed by oxidation of CH 3CN by metallic Pd and air, leading to cyclo(ortho)palladated complexes containing nitrite anion, e.g. Pd(NO 2)(C∧N)L (C∧N = papaverine; L = CH 3CN or DMSO) can be explained by Pd 3(OAc) 5NO 2 acting as the nitrite source. Finally, photocrystallographic metastable linkage isomerisation and complete conversion to an oxygen-bound nitrito complex Pd(η 1-ONO)(C∧N)PPh 3 has been observed.

    Details

    Item Type Articles
    CreatorsBajwa, S. E., Storr, T. E., Hatcher, L. E., Williams, T. J., Baumann, C. G., Whitwood, A. C., Allan, D. R., Teat, S. J., Raithby, P. R. and Fairlamb, I. J. S.
    DOI10.1039/c2sc01050j
    DepartmentsFaculty of Science > Chemistry
    RefereedYes
    StatusPublished
    ID Code29612

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